高效液相色谱法测定淤泥和土壤中双酚A、壬基酚和辛基酚

Determination of Bisphenol, Nonylphenol and Octylphenol in Sludge and Soil by High Performance Liquid Chromatography

建立高效液相色谱法测定土壤和淤泥中双酚A、壬基酚和辛基酚。样品采用超声波萃取,以体积比1∶1的正己烷和丙酮作为提取剂,体积比90∶10的乙腈和水作为流动相,经Supelcosil TMLC-PAH色谱柱(250×4.6mm,5μm)分离后荧光检测器检测,双酚A、壬基酚和辛基酚的荧光激发波长是227nm,发射波长为313nm,样品在6min中内完全出峰。该方法的线性范围在0.1～20μg/mL之间,在0.1μg/mL、0.5μg/mL和1.0μg/mL 3个浓度的添加水平下土壤和淤泥样品的加入回收率分别在83.7%～115.6%之间和94.3%～106.2%之间。该方法简单、快速和经济,可用于淤泥和土壤实际样品检测。

An analytical method based on high performance liquid chromatography （HPLC） with fluorescence detector （FLD） was developed for the determination of bisphenol A （BPA）, nonylphenol （NP） and octylphenol（OP） in sludge and soils. The ultrasonic technology was used to extract the target molecules from sludge and soil samples. Sludge and soil samples were soaked with hexane-acetone mixture. The mobile phase was a mixture of acetonitrile and water（90： 10）. After chromatographic separation on Inertsil ODS-P column（250 × 4. 6 mm, 5 um ）, HPLC-FLD chromatograms of analytes were recorded at 313 nm（λex =227 nm）. The analysis could be completed within 6 minute. The linear range of the method was from 0.1 ug/mL to 20 /lg/mL. The recoveries at 0.1 ug/mL,0.5 ug/mL and 1.0 ug/mL levels for soil and sludge were from 83. 7% to 115. 6% and from 94. 3% to 106. 2%, respectively. The method is simple, rapid and low-cost for the determination of bisphenol, nonylphenol and octylphenol in sludge and soil.